Preface

The advent of X-ray diffraction in the early twentieth century transformed crystallography from an area of scientific inquiry largely limited to physics, mineralogy, and mathematics, to a highly interdisciplinary field which now includes nearly all life and physical sciences as well as materials science and engineering. The atomic resolution structural information which is now routinely afforded by the combination of X-ray diffraction and crystallography is indispensable for the characterization of many modern materials, the interpretation of their function, and when applicable the rational improvement of their properties. Brighter X-ray sources and improved computing resources drive the evolution of new techniques for the characterization of increasingly exotic materials.

This book is a collection of works showcasing some of the most recent developments in the field of crystallography. The history of a scientific field seldom accompanies a field's most recent technical advances between the same two covers. This collection, however, commences with a search for the elusive single narrative of the history of crystallography. Kahr and Shtukenberg introduce the reader to the numerous works which have attempted to describe the evolution of the study of crystals. Ultimately, the authors conclude that the independent narratives of Ilarion Ilarionovich Shafronovskii and Curtis Schuh provide the most comprehensive accounts of the history of crystallography to date and are 'unlikely to be surpassed for a very long time.'

The second chapter deals primarily with recent advances in experimental techniques in the study of crystals. Synchrotrons and free electron lasers are now capable of producing X-ray beams many orders of magnitude brighter that those produced by conventional sealed tube and rotating anode sources. The extreme brightness of these sources has enabled experiments which explore matter under extreme conditions. The contribution by Legrand surveys a variety of new experimental apparatuses which allow researchers to use these bright X-ray sources to explore the effects of high and low temperature, strong magnetic fields, and high pressure on a wide variety of materials. Also described in this chapter are the details of the X-CHIP an impressive new tool which enables researchers to grow crystals, examine crystals and collect Xray diffraction data on a single substrate. Okitsu and coworkers detail remarkable instrumentation for generating multi-beam pinhole X-ray topographs of single crystals which might be used to solve the phase problem in protein crystallography. The final

#### X Preface

contribution of this section authored by Paradies and coworkers employs a wide variety of experimental techniques including X-ray scattering and diffraction as well as electron microscopy and diffraction on nanocrystals and crystalline colloids of Lipid A-diphosphate to unravel the structure of this biologically important molecule.

Crystals as functional materials drives the field of crystal engineering which seeks to create solid-state structures with targeted physical and chemical properties. The third chapter highlights recent developments in crystal engineering and begins with a survey by Patel and Benedict that explores the latest research in two exciting areas of applied single crystal materials science: photochromic materials and molecular semiconductors. Improving these materials through rational design requires a nuanced understanding of the molecular interactions which determine their structures. Haukka and coworkers examine halogen bonding in a variety of organic and inorganic single crystals and illustrate that this particular non-covalent interaction is a useful synthon in the design and synthesis of advanced functional materials. The submission by Gudavarthy and Kulp describes a method for creating chiral CuO films using chiral precursors and additives which may serve as enantiospecfic catalysts for the synthesis of chiral drugs or other important enantiomerically pure compounds. The chapter concludes with an extensive survey of crystal structures of organic compounds in which Pesyan describes structural helicity, hydrogen bonding, and additional noteworthy observations.

The book concludes with works exploring computations related to the field of crystallography. The submission by Stroz describes a precise yet highly compact computational algorithm for the description and determination of the crystallographic space groups. The inability to directly calculate atomic orbitals and their populations from multipole refinements, except for high symmetry cases, places limitations on the analysis of electron density distributions in crystals. Tanaka and Takenaka describe the method of 'X-ray atomic orbital analysis' that yields the aforementioned physical quantities through structure refinements based upon quantum mechanical atomic orbitals. Determining the three-dimensional structure of a biologically important molecule can be costly and time consuming. The final chapter by Zhang presents a practical and useful computational approach to produce the three-dimensional structure of Prion Amyloid fibrils.

I am grateful to all of the authors for their excellent contributions. I hope you enjoy this book and that it provides inspiration for exciting future experiments in crystallography.

> **Jason B. Benedict** Department of Chemistry University at Buffalo State University of New York, Buffalo, NY 14260-3000, USA

X Preface

contribution of this section authored by Paradies and coworkers employs a wide variety of experimental techniques including X-ray scattering and diffraction as well as electron microscopy and diffraction on nanocrystals and crystalline colloids of Lipid

Crystals as functional materials drives the field of crystal engineering which seeks to create solid-state structures with targeted physical and chemical properties. The third chapter highlights recent developments in crystal engineering and begins with a survey by Patel and Benedict that explores the latest research in two exciting areas of applied single crystal materials science: photochromic materials and molecular semiconductors. Improving these materials through rational design requires a nuanced understanding of the molecular interactions which determine their structures. Haukka and coworkers examine halogen bonding in a variety of organic and inorganic single crystals and illustrate that this particular non-covalent interaction is a useful synthon in the design and synthesis of advanced functional materials. The submission by Gudavarthy and Kulp describes a method for creating chiral CuO films using chiral precursors and additives which may serve as enantiospecfic catalysts for the synthesis of chiral drugs or other important enantiomerically pure compounds. The chapter concludes with an extensive survey of crystal structures of organic compounds in which Pesyan describes

A-diphosphate to unravel the structure of this biologically important molecule.

structural helicity, hydrogen bonding, and additional noteworthy observations.

structure of Prion Amyloid fibrils.

crystallography.

The book concludes with works exploring computations related to the field of crystallography. The submission by Stroz describes a precise yet highly compact computational algorithm for the description and determination of the crystallographic space groups. The inability to directly calculate atomic orbitals and their populations from multipole refinements, except for high symmetry cases, places limitations on the analysis of electron density distributions in crystals. Tanaka and Takenaka describe the method of 'X-ray atomic orbital analysis' that yields the aforementioned physical quantities through structure refinements based upon quantum mechanical atomic orbitals. Determining the three-dimensional structure of a biologically important molecule can be costly and time consuming. The final chapter by Zhang presents a practical and useful computational approach to produce the three-dimensional

I am grateful to all of the authors for their excellent contributions. I hope you enjoy this book and that it provides inspiration for exciting future experiments in

**Jason B. Benedict**

USA

Department of Chemistry University at Buffalo

State University of New York, Buffalo, NY 14260-3000,

**Section 1** 

**History of Crystallography** 

**Chapter 1** 
